반응식
[C:1]([N:8]1[CH2:12][CH:11]=[CH:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].BrN1C(C)(C)C(=O)N(Br)C1=[O:16].[C:24](#[N:26])C>>[OH:16][CH:11]1[CH:10]([NH:26][CH3:24])[CH2:9][N:8]([C:1]([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2])[CH2:12]1참가 물질
4
실험 절차
N-Boc-3-pyrroline (1) (16 kg) was treated with 1,3-dibromo-5,5-dimethylhydantoin (DBDMH) (15.2 kg) in aqueous ACN to form the bromohydrin (2). After the reaction was complete, the excess brominating agent was quenched with aqueous sodium thiosulfate solution and the crude reaction mixture was treated with aqueous NaOH. The resulting epoxide was extracted with MTBE and the organic layer was concentrated to give the crude epoxide (3). This epoxide was added to 40% aqueous methylamine and, after the reaction was complete, the excess methylamine and water were removed by distillation and the product, (4), (18.5 kg) was isolated from diisopropyl ether.
출처 및 근거
- ORD 기록
- ord-549df69d72d144ea8860d72d6bdf7831
- 출처 데이터셋
- uspto-grants-2013_07
- 특허 번호
- US08497282B2
연결된 노트
불러오는 중…